Automatic device for taking samples of active solutions



Sept. 12, 1961 A. REDON 2,999,738

AUTOMATIC DEVICE FOR TAKING SAMPLES OF ACTIVE SOLUTIONS Filed Aug f 26, 1959 2 Sheets-Sheet 1 Sept. 12, 1961 A. REDON 2,999,738

AUTOMATIC DEVICE FOR TAKING SAMPLES 0F ACTIVE SOLUTIONS Filed Aug. 26, 1959 2 Sheets-Sheet 2 I i a Q 0 I N ml H l l l T l ....1

I I :E F (\i I a: l\ g) i 55 L .J

Yum-u" i I J, 0 In i I I H 3" i l l l I.

is I 1 EU. N. m AL,

United States.

1 France Filed Aug. 26, 1959, Ser. No. 836,090

7 Claims priority, application France Aug. 26, 1958 6 Claims. (Cl. 23-259) In the course of chemical treatments of irradiated nuclear fuels the possibility must be provided of taking it possible. to take several successive samples, since the device returns to its initial state after each sample pre Y paring operation, which is eflected by a single action of samples of the aqueous active solutions, under conditions of maximum security.

I In effect the preparation of samples of such solutions (active or, B, 7) presents the problem of protection against radiation 8 and 'y rays) and contamination through the liquid (on, p and 'y rays).

' Known devices employed for this purpose comprise,

screens adapted to stop the rays, the operator controlling at a'distance the handling of the radio active liquid from behi'ndthe screen. 'However, such devices are not completely safe and a relatively large number of actions is required; The'pre'sent invention relates to an automatic device for taking samples of active solutions, which makes it possible to' reduce the number of actions and affords efiicient protection against radiation and contamination. i"-The device is essentially characterized by the combination of the following elements: j -"(l) :An electro-pneumatic motor system constituted on the one hand by a liquid switch which makes use ofthe contact of the active solution .with the conduit feeding the sample bottle, the movement of the solution which is subjected to a lowering of pressure caused by av single action of the operator, creating such contact" and at the same time causing the solution to enter the. feeding conduit;,and on hte other hand by a vacuum valve and by an atmospheric valve, closing of the-vacuum valve being effected by the above-mentioned contact and in turn causing the opening of the atmospheric valve, which efiects separation of the body of the solution and of the fraction which has penetrated into the feeding conduit, the combined movements of the two valves being determined in such a way that separation takes place at a given time, to; collect the desired quantity of active solution.

' (2) An external lead enclosure from which emerges the extremity of the feedingconduit, to which is adapted, during the taking of the sample, the bottle surrounded by a lead container, the enclosure and the container thus forming an assembly which ensures efiicient protection. r

. (3) A positioning device for the sampling bottle surrounded by the lead container which has a removable lid, the bottle enclosed by the container with its lid being brought to face the feeding conduit or removed from this position by means of a carriage, the lid of the container being removed when the bottle is subsequently adapted to the feeding conduit for'filling, and being replaced after this operation.

T (4) A safety device in case the system is not funct'ionin'g'properly, which makes it possible to return the system to its initial condition by interrupting the vacuum and bringing the enclosure to atmospheric pressure, the safety device being operated: g

(a) By a second tact of the solution when the contact with the feed conduit has not worked;

(b) By an action of the operator, for example, depression of a stop push button; QcLBy absence of current.

The device in accordance with the invention makes p in the reserve vessel is sucked into this enclosure and the operator.

The device also. makes it possible to empty the sampling bottle.

The sample bottle communicates through the feeding conduit With an internal enclosure which-holds the active solution. Preferably the feeding conduit consists at the bottle end of a hypodermic needle on which is stuck the bottle; this avoids any danger of contamination by the liquid. The enclosure communicates with a solution reserve vessel and is connected to a vacuum device through a first valve named vacuum valve," and to the atmosphere through a second valve named. "atmospheric valve."

:For protection against radiation the device is located inside an external lead enclosure, except for the end of the feeding conduit on which is adapted externally of the lead enclosure the sample bottle.

The vacuum valve and the atmospheric valve may be;

inside or outside the lead enclosure. The sample bottle,

during its displacements and during the taking of the sample, is always located in a protective lead container which, when thesample bottle is in place, forms with the lead enclosure an assembly ensuring total protection against radiation. When the sample bottle is displaced either to connect it ordisconnect it, the protective containermust be such as to assure complete protection; for this purpose it is provided with a lid. The latter is removed when the feeding conduit is adapted to the bottle. e

The vacuum circuit must enable the elimination of droplets of active liquid carried along during the sucking stage; this may be efiected by means of a guard vesselin the vacuum circuit. Thesample bottle, is preferably mounted in upside down position above theenclosure, the feeding conduit being vertical and the movement of liquid in said conduit being upward from the bottom, from the enclosure to the bottle.

When the sample bottle is adapted to the feeding circuit, the vacuum valve being closed and the atmospheric valve opened, the filling operation is started and carried out by a single action of the operator, which consists,

for example, in depressing a start push button of an electric panel. This action closes the atmospheric valve, which as soon as it is closed causes opening of the vacuum valve. enclosureinto which terminates one extremity of the feeding conduit.

exists in the-internal enclosure the solution contained arrives at the level of the extremity of the feeding conduit, thus establishing an electric contact; at this instant the solution starts to penetrate into the bottle-feeding conduit which is then under vacuum. The electric contact established by the solution causes closing of the vacuum valve. valve is closing, the atmospheric valve remains closed. The end of the closing movement of the vacuum valve controls opening of the atmospheric valve. Assume V to be the quantity of solution which has penetrated intoa certain time in contact with the extremity of the feeding tube after the atmospheric valve starts to open, a

' l atenlzed Sept. 1 9

A vacuum is created in the internal- The latter, as well as the bottle, is initially empty of solution. Due to the vacuum which- During all the time that the vacuum- If the arrangeuan i y a '3'; l ltiqllmay still penetrate into 'ndult s c u e by r flux f he-rat s of o ution to:

us: th rsssr ve el und r: th ef ect. o h pres: sure in the enclosure. The quantity of solution V which has penetrated into the feeding conduit is subjected on theone hand to the atmospheric pressure in the en; closure and on the other hand to the vacuum in the bottle. This quantity'flows into the bottle wherein itis retained, and opens the feeding conduit, which brings thebottle back to normal pressure.

A conventional electric circuit assembled on a con t'rol panel remote from the samplepreparing device and comprising a suitable relay system, makes it possible to control: 4

11 Closing of the atmospheric valve bythe initial action of the operator; n

Opening of the vacuum valve .ajt the enrl of closing of the atmospheric valve;

, Closing ofthe vacuum valve by contact of the liquid with the extremity of" the feeding conduit;

Opening of the atmospheric valve at the end of cloak-- ing of the vacuum valve.

A-safety system isprovided in case the device does not function properly; the latter thus comes back to -itsand the sample bottle 3 sealed by a rubber stopper; of h .3 .11 We as P n c n b l with t ed n on.- duit 4 terminated by a hypodermic needle 5 on which is stuck the bottle 3. The feeding conduit 4 is electrically insulated from the enclosure 2 by a plug 6. A high e probe el ctrically ns a d from the en l sure 2 initialcondition by interruption of the vacuum and by return of the enclosure to atmospheric pressure.

The safety system. is put into operation: I (1) By a second contact of the liquid Wildflthfiobtk; tact oi the liquid with the feeding circuit'has not worked.

"(-2) By the action of the operator. for -example, is stop push button.

3 3) By absence of cur-rent. The combined movements of thetwo valves erode termined in such a way: that separation:- off the mass of and ofthe-fracti'on which has entered in' the corn duit takes place at a suitable moment to collect-in the bottle the desired quantity of liquid.

' s quantity 1S' furthermore also a function of sevoral factors sueh as the diameter of the feeding conand the amount" of 'va'ouum. After a filling oper ation the valves comeback to their-- initial position, name ly, the atmospheric valve opens and the vacuum valvecloses, so that a new isample may be taken by substituting for; the bottle which has been filled; an empty bottle.

the filled bottle is left in position of; a second manoeuvre of the operator with the same control of the electric panel results in emptying of thebottleby'suc tion of. its contents, if the communication normally existing during filling between the internal enclosure andthe reserve vessel is shut off,

;-It is; thus possible to carryout automatically filling;

and emptying operations of. sample; bottlesu'nder security conditions. 7 'A non-limiting embodiment of the automatic device for taking samples oi active solutions in accordance with the invention will nowbe described with reference to the accompanying schematicaldrawing.

The particular 'features described with reference to said embodiment are to be considered as part of the in vention, it being understood that any equivalent arranges ments may be made use; of within the-scope 0t the-in vention.

FIGURE 1 represents an automatic devicefortaking ples of active solutions; in accordance: with them vention. Y

FIGURE 2- is: a diagram of; the electrigcontrol panel. of 'said device; the. panel is-out's'ide the lead enclosure" and remote from the device. a I

Corresponding elements of'h different figures are indicated by the same reference characters".

enclosure 2- whichreceivesthe liguid frorn the vessel-{ FIGURE-1 shows the reverse vessel' 1; the internal by a plug 8 makes its possible to establish a contact beween th acti e lution and t P n, e ontact bet e n theact ve ol io nd. the feedin u 4 ha not functioned. A vessel '9 constitutes a guard on the vacuum circuit and makes it possible to remove droplets f m he rhich. hasb en, su k d n An; electr magnetic valve 1! controls the evacuation of the enclosure 2 and an electromagnetic valve 11 places the enclosure in communication with the atmosphere. Shown very schematically in the. drawing are the electro-.- magnetic windings of valves 10. and 11, indicated res spectively at 12 and 13. The vacuum valve 10 com! prisesv a switch 14 whichis-opened only when the valve is completely closed. The atmospheric valve 11 com prises a switch 15 which is closed only when the valve is completely closed. A- conducting wire 16? connected to 'the'portion of the feeding circuit 4 situated between the bottle 3 and the enclosure 2 and connected to the upper extremity of. the probe 7, ends in a terminal A. A conductor 17 connected to the enclosure 2 ends in a; terminal B.

The terminals A and B, as well as the terminals or? windings 12 and 13, and of switches 14 and 15, are'connected. to the controlpanel.

' A shut-elf valve 18'is placed in the conduit of-the solution betweenthe reverse vessel 1 and the-enclosures 2; This valve: remains always open when samples; are taken, and it is closed when the. bottle 3 is drained; the valve is controlledfrom the outside manually orautomatically.

The device. is protected by a lead enclosure: 19. valves 10 and 11. are. outside the enclosure. When the: bottle 3 is not in place the needle: 5, which is. designed}- to be stuck into the-bottle 3, projects externally of the enclosure. Thebottle is inside alead container20. lid- 21 of: container 20 is shown on a; carriage; 22; there; is also shown a lifting device. 23.

The enclosure 2-, the feeding conduit 4. the probe: 7-;- the-vacuum guard vessel and the connection tubing are of very low'ca'rbon 1.8/8 stainless. steel. The insulating plugs and 8- are of Teflon (tetrafiuoroethylene'resin; trademark owned by E; I. duPontde- Nemours & Co.).

The device is used for'taking samples of concentrated: solutions of fissionproducts, resulting from the treatment of irradiated fuels.

The sample bottle 3 isplaced in the lead container 20. The latter is mounted upside. down on the carriage 22 which carries it under the lifting device 23. lathe-first place the, container 20 is lifted to permit removal of the lid 21;. the carriage 22 supporting the lid 21 is moved? aside. The container is lowered so as to stick the bottle 3 .on the hypodermic needle 5. The bottle 3 is thus in the position required for the taking, of'a sample. Filling; of 'the bottle is carried out as follows:

The shut ottgvalve 18 and the atmospheric valve, 1 1' being Qpent he acuum. alve 1Qbe ng.,c dith mpl bottle. 3 surm udedbv t contai r. eing s u k n h hypodermic needle 5, action of the operator on apush button of the control panel causes closure of the stripesnhs c al e 1... B li g. hen. takes. place. automa ic lly; theend'ofthe closingmovement of thezatmospheric v lve 11; causes by' theintermed atfy. Qiihfi. sw tch. l fl illsl of'the vacuum valve 10 and evacuation oiair frornthe en} closure 2 and the bottle 3. The liquid in the reserve 1 is suckedup and rises in the enclosure 2; contact of the liquid withthe lower extremity 24 of the feeding;: conduit 4 closes the electric circuit between A and B through the circuit including conductor 16, feeding conduit 4, the liquid, enclosure 2 and conductor 17; this causes closure of the vacuum valve the end of the closing movement of said valve eifects through the action of switch 14, opening of the atmospheric valve 11.

Up until the opening of the atmospheric valve 11, the bottle 3 and the enclosure 2 are under vacuum; when this valve opens the vacuum is suppressed and a certain quantity of liquid has already risen in the feeding conduit 4; this conduit may still receive some liquid after opening of the atmospheric valve 11; at a given moment there takes place separation of the body of liquid from the fraction which has risen in the feeding conduit 4. The bottle 3 being then at a lower pressure thanthe enclosure 2, all the liquid which has risen in the feeding conduit 4 is forced into the bottle 3. This liquid is retained in the bottle. The feeding conduit is then opened and the bottle is brought to atmospheric pressure. The container 20 is lifted, the carriage 22 is moved under the container 20, which is lowered on its lid 21. The operator fastens the latter by means of two bolts. The sample taking operation is finished. The situation is then the same as at the beginning and the operation may be repeated by adapting a new sample bottle.

To empty the bottle 3 which contains a sample, the atmospheric valve 11 being opened and the vacuum 10 being shut, the shut on? valve 18 is closed and the same push button of the electric panel, which has been used to eifect filling, is depressed; the liquid of bottle 3 is then sucked into the enclosure; after having closed the vacuum valve 10 and opened the atmospheric valve 11 it is suflicient to open the shut oif valve 18 to obtain flowing of the drained liquid into the reserve 1. There is only left in the bottle 3 a drop of liquid due to the projecting of the needle 5. If during filling the contact between liquid and feeding conduit 4 does not function normally, the liquid arriving in contact with the lower end of the high level probe 7 causes suppression of the vacuum and return of the enclosure 2 to atmospheric pressure.

FIGURE 2 shows relays 25, 26 and 27, two push buttons start '28 and stop 29 and the terminals A and B. There are shown also the windings 12 and 13 shown less schematically than in FIGURE 1, and the switches 14 and 15. I

Before commencing the filling operation the elements of the electric panel are in the following conditions: Relays 25, 26 and 27 not energized, winding 12 not supplied with current (which corresponds to valve 10 closed), winding 13 not supplied with electric current (which corresponds to the atmospheric valve 11 open) switch 14 open, switch 15 open, switch AB open.

Control of the electro pneumatic motor system from the electric panel is effected in the following manner: the sta push button 28 energizes relay 25 which through the intermediary of winding 13 which is thus supplied with current, controls closing of the atmospheric valve 11. When this valve reaches the end of its course, the switch 15 closes and energizes relay '26 which by the intermediary of winding 12 which is supplied with current, controls opening of the vacuum valve 10. Opening of the latter valve causes closing of the switch 14. When contact is established by the liquid between the enclosure 2 and the feed conduit 4, the relay 27 is energized and opens the supply to relay 25 which has the elfect of closing the vacuum valve 10, through the intermediary of the winding 12 which is no longer supplied with current. For the duration of the closing movement of valve 10, the switch 14 which is closed, keeps winding 13 supplied, and thus keeps the atmospheric valve 11 shut. As soon as the vacuum valve 10 is completely closed the switch 14 opens and cuts current supply of the winding 13, and the atmospheric valve 11 opens; the beginning of the opening movement of the latter valve eifects opening of the switch 15 and de-energizes relay 26. The opening of contact AB due to the movement of the solution eifects d e-energizing of relay 27. All the elements of the control panel have thus returned to their initial condition.

The operation of the stop push button 29 has the same result as energization of the relay 27, namely suppression of the vacuum and communication of the enclosure 2 with the atmosphere.

The electric circuit is 'fed under 24 volts. The electric panel is remote from the sample taking device.

The embodiments of the invention in which an exclusive property or privilege is claimed are defined as follows:

1. In an automatic device for taking samples of active solutions, a sample bottle, a conduit feeding said bottle, means for placing said solution under vacuum, single action control means for said vacuum means, an electro-pneumatic motor system, a liquid switch actuated by contact between the active solution and said feeding conduit in said system, said vacuum means causing said solution to contact and enter said feeding conduit, a vacuum valve and an atmospheric valve in said system, means for closing'said vacuum valve actuated by contact between the solution and said conduit, means actuated by closure of said vacuum valve for opening said atmospheric valve whereby the body of the solution is separated from the fraction of the solution which has penetrated said feeding conduit to collect a desired quantity of the active solution in said bottle.

2. In a device as described in claim 1, an external lead enclosure for the device, said feeding conduit passing through said enclosure, and a lead container for said bottle, said bottle being mounted on the end of said feeding conduit during the taking of a sample, said enclosure and said container forming a protective assembly.

3. In a device as described in claim 1, a lead container for said bottle, a removable lid for said container, and means for mounting said bottle on said feeding conduit including a carriage supporting said container, said lid being removed from said container when said bottle is mounted on said feeding conduit for the filling of said bottle, said lidbeing replaced on said container after filling of said bottle.

4. In a device as described in claim 1, a security systern operative on malfunction of the device including means for breaking the vacuum and for placing the solution under atmospheric pressure to return the system to its initial condition and electrically actuated control means for said last named means including a second electric contact engaged by the solution when the contact between the solution and said feeding conduit is inoperative and a manually actuated electric switch.

5. In a device as described in claim 1, means for returning said electro-pneumatic motor system to its initial state after each sample taking operation.

6. In a device as described in claim 1, means for draining said bottle actuated by said single action control means.

References Cited in the file of this patent UNITED STATES PATENTS 

1. IN AN AUTOMATIC DEVICE FOR TAKING SAMPLES OF ACTIVE SOLUTIONS, A SAMPLE BOTTLE, A CONDUIT FEEDING SAID BOTTLE, MEANS FOR PLACING SAID SOLUTION UNDER VACUUM, SINGLE ACTION CONTROL MEANS FOR SAID VACUUM MEANS, AN ELECTRO-PNEUMATIC MOTOR SYSTEM, A LIQUID SWITCH ACTUATED BY CONTACT BETWEEN THE ACTIVE SOLUTION AND SAID FEEDING CONDUIT IN SAID SYSTEM, SAID VACUUM MEANS CAUSING SAID SOLUTION TO CONTACT AND ENTER SAID FEEDING CONDUIT, A VACUUM VALVE AND AN ATMOSPHERIC VALVE IN SAID SYSTEM, MEANS FOR CLOSING SAID VACUUM VALVE ACTUATED BY CONTACT BETWEEN THE SOLUTION AND SAID CONDUIT, MEANS ACTUATED BY CLOSURE OF SAID VACUUM VALVE FOR OPENING SAID ATMOSPHERIC VALVE WHEREBY THE BODY OF THE SOLUTION IS SEPARATED FROM THE FRACTION OF THE SOLUTION WHICH HAS PENETRATED SAID FEEDING CONDUIT TO COLLECT A DESIRED QUANTITY OF THE ACTIVE SOLUTION IN SAID BOTTLE. 